顶空毛细管气相色谱法测定龙胆泻肝片中残留溶剂
Determination of Residual Solvents in LongdanXiegan Tablets by Headspace Capillary Gas Chromatography
尹兴章 1谭冬梅 2张远溪 3赵一丁 3杨深应 1王健芬1
作者信息
- 1. 保山市食品药品检验检测中心,云南 保山 678000
- 2. 云南经济管理学院,云南 昆明 650000
- 3. 保山中医药高等专科学校,云南 保山 678000
- 折叠
摘要
目的:旨在建立一种新方法测定龙胆泻肝片中甲醇、乙醇的有机溶剂残留量.方法:采用顶空毛细管气相色谱法,色谱柱为安捷伦 DB-624 毛细管色谱柱(30m×ϕ0.53 mm,3 μm);检测条件为:程序升温;进样口温度为220℃;检测器(FID)温度为250℃;分流进样,选择5∶1 的分流比;顶空瓶平衡温度85℃,平衡时间20 min.结果:甲醇、乙醇两种有机溶剂分离效果良好,分别在1.0335～248.04 μg·mL-1(r=0.9997)、1.0505～252.12 μg·mL-1(r=0.9996)范围内有与峰面积良好的线性关系,平均回收率分别为97.4%(RSD=1.7%,n=6)、95.7%(RSD=1.6%,n=6).结论:方法重复性、精密度和回收率较好,而且操作简便、灵敏度高、选择性强,可为龙胆泻肝片残留溶剂质量控制提供参考依据.
Abstract
(Objective)The aim is to establish a new method to determine the organic solvent residues of methanol and ethanol in Longdan Xiegan tablets.(Methods)Headspace capillary gas chromatography was used,and the column was an Agilent DB-624 capillary column(30 m×ϕ0.53 mm,3 μm);the detection conditions were:programmed temperature rise;inlet temperature was 220℃;detector(FID)temperature was 250℃;split injection,5∶1 split ratio was selected;headspace vial equilibration temperature was 85℃,equilibration time was 20 min.(Results)The two organic solvents,methanol and ethanol,were well separated with good linearity in the ranges of 1.0335～248.04 μg·mL-1(r=0.9997)and 1.0505～252.12 μg·mL-1(r=0.9996),respectively,and the average recoveries were 97.4%(RSD=1.7%,n=6),95.7%(RSD=1.6%,n=6).(Conclusion)The method has good repeatability,precision and recovery,and is simple,sensitive and selec-tive,which can provide a reference basis for the quality control of residual solvents of gentian diarrhea liver tablets.
关键词
龙胆泻肝片/甲醇/乙醇/残留溶剂/顶空毛细管色谱法Key words
Longdan Xiegan Tablet/Methanol/Ethanol/Residual Solvent/Headspace Capillary Gas Chromatography引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据